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超高效液相色谱-串联质谱测定蔬菜鲜样中喹诺酮类抗生素

etermination of quinolones in fresh vegetable using ultra-high performance liquid chromatography-tandem mass spectrometry

中文摘要英文摘要

建立了超高效液相色谱-串联质谱 (UPLC- MS/MS)测定蔬菜鲜样中4种喹诺酮类抗生素的分析方法。称取5 g研磨后的蔬菜鲜样以10 mL乙酸-乙腈(1/100,V/V)进行涡旋-超声提取,用HLB固相萃取柱进行净化富集,以4mL乙酸-乙腈(1/100,V/V)进行洗脱。以0.1%甲酸乙腈溶液和0.1%甲酸水溶液作为流动相,采用梯度洗脱方式进行UPLC-MS/MS分析。蔬菜中4种喹诺酮类化合物的加标回收率为83-102%,相对标准偏差(RSD)为0.8-8.0%,检出限为0.003-0.199 μg/kg,定量限为0.009-0.662 μg/kg。对广州市蔬菜进行分析结果表明,该方法能够满足实际蔬菜样品的分析要求,蔬菜中喹诺酮类抗生素污染问题值得关注。

n analytical method for determining four quinolone antibiotics in fresh vegetable using ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed. Five gram of ground fresh vegetable sample was extracted using 10 mL of acetic acid-acetonitrile (1/100,V/V) under vortex- ultrasonic treatment.The extract was purified and concentrated by HLB cartridge, followed by eluting the HLB cartridge using 4 mL of acetic acid-acetonitrile (1/100,V/V). Using 0.1% formic acid in acetonitrile and 0.1% formic acid as the mobile phase, the analyte was determined with UPLC-MS/MS under gradient elution approach. The recoveries of four quinolone compounds in fresh vegetable samples were from 83% to 102%, with relative standard deviation (RSD) less than 10%. Limit of detection and limit of quantification ranged from 0.003 to 0.199 μg/kg and from 0.009 to 0.662 μg/kg, respectively. The analytical method was successfully used to determine four quinolone antibiotics in fresh vegetables from supermarkets of Guangzhou city, which suggested a health concern related to pollution of quinolone antibiotics in vegetable.

高增霞、莫测辉

植物保护环境污染、环境污染防治生物科学现状、生物科学发展

蔬菜鲜样喹诺酮类抗生素超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法

vegetablefresh samplequinolone antibioticsUPLC-MS/MSanalytical method

高增霞,莫测辉.超高效液相色谱-串联质谱测定蔬菜鲜样中喹诺酮类抗生素[EB/OL].(2012-06-05)[2025-08-02].http://www.paper.edu.cn/releasepaper/content/201206-86.点此复制

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